Sealing composition



' a te in. 1a, 194s f smtmooom osmou Laurence Rector, Fort. Worth, and Charles L.

- Cron, Houston, Tex:

No Application Mini. 10, 1941, ;Serlal No. stasis J v 14 01. 106-171) i I This invention relates to new and: useful im-' provements in sealing compositions.

' This application is filed as a continuation-inpart of our co-pending application, Serial No. 281,828, filed June 29, 1939.;

One object.. of the invention is to provide an improved sealing composition for sealing contacting metallic surfaces or-Joints and being'particularly adapted" for use in sealing screwthreaded joints, whereby leakage-past the joint is prevented; the composition also being' applicable to gaskets, or, other sealing elements for enhancingtheir sealing efl'lcienc'y. 3

"A particular object of theinvention is to'provide an improved sealing composition which is waterproof and is also unaffected by petroleum,- or any of its fractions, and which will maintain its. seal i qualities under the action of salt water, dilute acids, and other corrosives occur ring in c'rude'oil, thereby making it particularly A useful in the petroleum industry, although it ma be used elsewhere? "An. important object of the invention is to provide an improved sealing composition having a Another object ofthe invention is to provide a'com'position, of the character described, which includes a base solution consisting of a cellulose derivative dissolved in a group of liquid solvents,

5 such as esters and ketones, the solvents having boiling points which vary from low to high over a given range,'whereby when evaporation occurs,

the rate of evaporation is uniform and gradual, with the result that the composition changes from its .original free flowing consistency to a plastic mass which will-not flow of its own accord or under considerable pressure, and the solution 1 will not become dry or brittle because of evaporation, as wouldbe the case if only one solvent of f a low boiling point was employed.

' A still further object ofthe inventionis to providean improved sealing composition wherein the base solution has a softener or plasticizer admixed therewith in exces point of the final state of the'composition, where by upon standing or aging,the excess plasticizer will slowly exude from the composition to provide .a protective film of lubricanton theesurface of sive amounts: that is, the amount-oi plasticizer exceeds the retentivity said composition, the lubricantbeing desirable" consistency which facilitates its application to a particularly when 'the composition is employed metallic-or other surface and which, after stand ingfsets in a soft-pliable mass which maintains on screw-threaded Joints. elasticity and mobility to a degree, whereby it In producing the improved' composition, any neverhardens to a brittle stage and; therefore. derivative-of cellulose, such as asalt (cellulose does notinterfere with'the-breaking of'the jbint nitrate), an organic ester (celluloseacetate) or 7 at any time after application of the-composition,

regardless of the lengthj'oi'j time-thatsaid conipositionmay have been applied.

- an improved; sealing composition or compound.

" -form'a coating of lubricant betweenth'e surface of, the composition and the surface of the inetal r to which it is applied, whereby breaking" ordis-. I

connection of the joint is' facilitated.

I'Y. further object'of the invention is to provide an improved sealing composition consisting of cellulose de 'ivmive villi-i011 adm xed with a solution softener. such 21: vegetable oil,and an inert solution containing about twelve per. cent of the cellulose. derivative has a'suitableconsistency, but

the invention is notto be limited to, this figure as mineral'filler, the constituents being in-su'ch proportions as to produce a substance having a relameans of a brush or swab.

- Another object of the invention is to provide ,an ether (ethyl cellulose or benzyl cellulose) is that any derivative of cellulose may be substituted therefor.

.The cellulose nitrate is dissolved in 'a liquid solvent'or group of solvents, the dissolution being -effected during thorough'agitation or mixing. 49, Theliqui'd solvents may be esters and ketones,

which vary in boiling points overyfa relatively wide range; as for -examfle'fi'rom degrees to.300 degrees FLY As explained, the cellulose nitrate is dissolved in this group of solvents to form '4 a base-solution and the proportion'ot the jcellu 'losederivative to the solvents is such that said olution has bodysbiit is quite mobile, being ca pable of-flowing; It. has been found that a base purpose of the invention.

, boiling solvents.

The base solution so formed is made up of a cellulose derivative in solution in a series of solvents. This series of solvents 'ranges in boiling points from a fairly low temperature, 50to 100 solvents having the lower boiling points, will.

evaporate from the composition allowing it to harden somewhat. However, the solvents present that have a high boiling point will not evaporate even under considerable heat, and theymaintain thecomposition in an elastic dition. It will be seen that the fi al or terminal consistency of the composition maybe determined beforehand by varying the proportions; of the lighter and. the heavier solvents. Also, it is obvious that the composition will not become caked-or brittle, but will be held in an elastic condition indefinitely by the action of the high The elasticity of the compound is not sunlcient as to allow it to fiow of its own accord or under pressure, but it is sufilcient as to prevent the compound from 'caking or chipping However, after the composition has set, and'the solvents have partially evaporated, no ingredient remains to retain the castor oil so that it separates and exudes slowly from the mass oi the composition. Any softener used in this composition is used in such amounts as to exceed the retentivity point of-the particular cellulose derivative for that softener. Y

The oil or softener is added to the base solution preferably in an amount equal in weight to the weight of the base solution, although these proportions may vary. When added in an amount equal in weight to the weight of the base solution,

d plastic cona, ratio of softener. or oil-to the cellulose nitrate of approximately eight to one exists, but it is pointed out that this figure is illustrative only. Although the'exact amount of softener or plas ticizer which is added tothe base solution is subjectto variation, it is desirable that sufficient softener or plasticizer be added so as to exceed the point of retentivity of the cellulose nitrate.

Thus, when the mixture is allowed to stand, the softener or plasticizer slowly exudes from the mixture. This exuding plasticizer, which is the vegetable oil, forms a thin protective film on the outer surface of the compound, as will bemore fully explained. The excess plasticizer is carried under conditions of vibration. The higher boiling solvents used are preferably non-soluble inpetroleum or its fractions. Thereby, the compound may'not be dissolved or disintegrated by said petroleum, and is-ideal for usein oil well tubing and casing and machinery Joints.

The base solution, consisting of the cellulose nitrate and the group of solvents, is then admixed with a plasticizer or softener, the latter being preferably added to the solution while stirring. The plastlcizer or softener is on of very low solubility in petroleum hydrocarb ns and one which is non-drying and has lubricating qualities. It

has been found that a vegetable oil, and particularly castor oil, issuitable. Castor oil is nondrying; has high lubricating qualities, is of low solubility in petroleum hydrocarbons, and is compatible in limited proportions with cellulose nitrate. If added suddenly to the base solution, castor oil might result in curdling or precipitating the cellulose nitrate and, therefore, to avoid I this, it is desirable that the castor on be added slowly and with stirring. It ispointed out that the invention is not to be limited to castor oil and a point of nitrocellulose for castor oil is reached when approximately five times as much castor oil as nitrocellulose. by weight, has been addedto the nitrocellulose. Thus, castor oil in excess of this amount may not be retained by the nitrocellulose in a-homogeneous phase.

The solvents added tothe nitrocellulose will retain the castor oil which has been added in excess ofxthe retentivity of the nitrocellulo e-- in the-composition in minute particles muchas the oil' is carried in a stable oil-water emulsion This suspension is very stable and the plasticizer I does not commence to exude or sweat out of the compositionv until the composition has lost part of'itssolvents by evaporation and has hard ened to its final state. The addition of the vegetable oil does not materially change the consistency of the original base solution and functions in the compound to prevent drying beyond a given or predetermined point and also functions as a lubricant.

After the base solution and softener or plasticizer (castor oil) are,admixed,;a suitable bull:- ing agent, such as a mineral filler, is added. The filler is inert, insoluble in water, petroleum, salt water and dilute acids. The filler is preferably added in amounts sufficient to give the mixture a thick consistency substantially that of molasses. It has been found that such consistency is obtained by adding the filler in amounts equal to from fifty to eighty per cent of the total weight of the liquid, depending upon the density of the filler used. Although any suitable mineral filler may be employed, a filler, such as .asbestlne,

clay, graphite, talc,'or the like, may be employed. It is preferable that the filler be finely ground 1 so as to give the mixture a smooth texture. The

viscosity and specific gravity of the mixture is controlled by the amount and specific gravity of the filler. A mineral filler has been found entirely. satisfactory, but other equivalent fillers capable lot the same function in the composition, such aswood pulp, could be used. The mixture has a consistency substantially thatof molasses and is readily applied to a metal, or other surface, with a swabor brush. 7

In order to prevent the mineral from ettling in the liquid during storage, a suitable suspending agent, such as aluminum stearate, magnesium -lExamples illustrating the invention renew: v Percent-by wei ht Ethyl acetate 7.5 Example I Butyl acetate 2.5

. Amy! acetat 1,

,Benzol 6.5 .233}? Toluola I 2.5 Butyl alnnhnl 1 i iti 0e ttin assassin:-11-: 1 5., m0

i i iited solubility plastlclzer....- z 1 v 1. velezue bl-ll'fi'r'thiifieltifii" v In use; the composition is applied to the surface LiqudmMmQsmhnmmQ a of the extremities of the pipes, or other memv 100.0 bers to be joined, by means of a brush or swab. As explained, the composition is particularly adapted for sealing threaded joints, although it.

Example If may be used on gaskets or other elements. when applied to threaded joints, a layer or coating of f v 'the composition is applied to the threads. The

\ Parts by Pam, coating is sufficiently soft to permit the threaded 3 joint to be made up and said composition acts as a lubricant to' preventinjury to the joint due to ns le ofciflmlmmon after i l 1 7 frictional heat. After a period, the composition. ".8 .,Zi{ "fff 1:31:11; 5 which has filled the grooves formed by the threads, l i n 6 sets by evaporation. of the lighter solvents to a Qiififlgffffifi 0 3, soft pliable mass that is not mobile andwill not 4 m o 2. --fiow of its ownaccord or under considerable pressure, The presence of the plastioizer or softener in the composition aids in preventing the dryin of the'composition beyond a given point so that zxamplje'ifi I the same cannot dryto hardness. The group of i solvents, and the castor oil, in which the cellulose nitrate is dissolved, prevents the composition from 1:32,? Percent drying completely. As explained hereinbefore the composition dries to a hardened but elastic I I state, which allows it to be distorted and. prevents tifittffffff-ffffff'.Efffffifffiiiiii:111:: it it? conditions of s r vibrations Thus. the

Volatile portion of composition: position maintains a'- fiuid and pressure-tight seal Liquid 6 at the joint at all times and under all conditions.

' 100.0 As has been previously pointed out, the softener' or plastici'zer (castor oil) is admixed with the base solution in an amount which is in excess of the Example IV retentivity point of the cellulose nitrate. -when .the composition is applied to the joint and allowed to stand, the excess of the plastlcizer slowly Pal-Baby Pmnt exudes from the compound and such exudation "8 forms a thin film of said plasticizer, in this instance, castor oil, between the surface of the comai fg figlg 5mm? 5 pound and the surface of the metal. This film or ga actoil 5.111111" g 50 foatinglofithe calsitoruoil. which has hghlgbricat lug qua t es,'ma es possi e to rea ily reak or- 'tgiug'if f ffffiififffiii: s m a unscrew the Joint, regardless of the length of time Bumwmd 3 which said joint-has been made up; also, the film s 106.0 of oil, acting as a lubricant, reduces friction andprevents injury. to the threads by frictional heat..

. v The composition has been found particularly Example V adaptable for use in the petroleum industry as it ,is .substantially unaifected by dilute acids, gas.

x Per cent by wei ht gasoline or-other petroleum hydrocarbons; it is -Cellulose-nitrate- 4 also waterproof and is capable of withstanding Y Acetone 5 8.5 high pressure, as well as high temperatures. Al-

Ethyl acetate 10 though it has been used satisfactorily in the pe- Butyl ta: 2.5 troleum industry forsealing, threaded joints,

yj acetafp- 1 metal tank joints, and other'contacting' metallic Castor nn v 30 surfaces.v it may beused elsewhere. The con- Filler (Asb'estine) 44- (w stituents in the composition are insoluble in water, as well as insoluble in petroleum, as above 0 ,0 explained, and thereby form an efiective sealing composition forwater lines.

Example W This composition may also be made from cel- & iulose ethers,- such as ethyl cellulose or butyl c'el- Itereeatbyweisht lulose. The composition made from these, in-

' cellulose nitrate 4 radients is Very similar in every detailto'the c m;- 3 30 composition described hereinbeiore. In place of Filler (Asbestlne) .i

'7' the castor oil, a partially solvent softener. such as butyl stearate, is used;

Examples of this form of the invention follow:

' Example VII Parts by weight Percent Ingredients of composition after setting:

. Cellulose ether 2 6. 7 Limited solubility softener. 10 27. 7 Filler 12 33.3

Volatile portion of com osition:

Aromatic hydrocar ons and aliphatic sl- -coho l2 33.3

Example VIII Parts by weight Ingredients of composition after setting:

Ethyl cellulose 2 5. Butyl stearate 10 27. Fille 12 33. Volatile portion of composition Ethyl cohol 2 5. Toluol 10 27.

The proportions are such that the composition has a consistency substantially that of molasses,

' whereby saidcomposition may be readily applied to the surface to be sealed with a bruslior swab. This composition has all of thequalities or the first composition described herein and provides Butybstearate is compatible with ethyl or butyl cellulose in limited quantities, such as castor oil is in nitrocellulose.

stearate will exude from the composition after it has set. l

Another example is:

Although it is desirable to form the bases0lu-- tion by dissolving the cellulose derivative in a Thus, the excess of butyl,

group of solvents, as above explained, it would be possible to produce the composition 4n another manner. In place of the base solution as formed, above, commercial pyroxylin cement, which may,

be purchased on the open market, may be employed. There are various types of commercial pyroxylin cement on the market, but such cement consists of pyroxylin, which is a nitrocellulose; a solvent, such as ester, alcohol or ketone; a nonresin, such as shellac; and a plasticizer, such as an ester or ketone having a very high boiling point.

"The various types of pyroxyli'n cements onered solvent, such as benzene, xylene, or toluene;.a I

for sale on the open market may have the-pro;

portion of the substances thereof varied slightly,

7 wherebyslight variations in viscosity andother conditions or the cement may occur in such various commercialproducts. -,Also some of the ocmerits may not include the exact substances out lined above, and .it is pointed out that any prroxyli'n cement may be employed, provided it has the necessary characteristics outlined hereinbefore. i

In forming is admixed with a plasticizer andjlller mixture to form the sealing composition, The plasticizer described above, namely; castoroiland a suitable mineral filler, such as "asbestine." maybe 'used.

the mixture, the pyroxylin cement ,condition.

k plastic condition. q

. to the celluloseester.

a fluid and pressure-tight seal.

What we claim and desire to secure by Letters Patent is: v

1. As'ealing-composition including, a cellulose ether in physical solution-in a liquid solvent, a plasticizer physically soluble in the ether in lim- "ited proportions dissolved in the'ether solution in excess '0! its solubility in the ether, whereby when the liquid solvent evaporates, the excess of the plasticizer will separate from the ether and form a film of plasticizer upon the mass of the composition, while the balance or the plasticizer will remain intimately associated with the ether and maintain the mass of the composition in a 7 plastic condition.

2. A sealing composition including. vethyl cellulose in physical solution in a liquid solvent, a.

plasticizer physically soluble inthe ethyl cellulose in limited proportions dissolved in the ethyl cellulose solution inexcess of its solubility in the ethyl cellulose; whereb whenthe liquid solvent evaporates,the excess 0 the plasticizer will separate from the ethyl cellulose and form a illm of plastlcizer upon the .mass of the composition, while the balance or the plasticizer will remain intimately associated 'with the ethyl cellulose and maintain the mass or the composition in a plastic 3. A sealing composition including, a cellulose este'r in physical solution in a liquidsolvent, a

plasticizer physically solublein the ester in limited proportions dissolved in the ester solution in excess of its solubility-in the ester and in excess of the ratio of 5to'1' relatiye to said ester where- I by when the liquid solvent evaporates, the excess or the plasticizer will separate from theester and form a film of plasticizer upon the mass or the composition, while the balance or the plasticizer will remain intimately associated with the ester and maintain the mass 4. A sealing composition including, a cellulose ester in physical solution in a liquid solvent, cas- -tor oil physically dissolved in the ester solution. in excess of the retenti'vity of the ester for the castor oil, whereby when the liquid solvenifevaporates, the excess of the castor oil will separate from the ester and form a lubricating film of castor oil upon the mass 0! the composition, while the balance or the castor oil will remain intimately associated with the ester and maintain themass of the composition in a plastic condition.

5. A sealing composition including, a cellulose ether in physical solution in a liquid solvent, butyl stearate physically dissolved in the ether solution in excess of the retentivity of the ether for the butyl stearate; whereby whentthe liquid-solvent evaporates, the excess or the butyl stearate will separate from the ether and form a lubricating film or butyl stearate upon the mass or the composition, while the balance of the butyl stearate will remain intimately associated with the ether and maintain the massof the composition in a plastic condition. Y

6. A. sealingcomposition as set forth in claim '4 wherein the castor oil is present in the composition in excess of the ratio of 5 to 1 with respect 7. n sealing composition including a mixture of the composition in a Amyl acetate 8. A sealing composition including a mixture I oi the following ingredients in the approximate proportions stated:

t??? Percent F1119! 6 33. Ethyl acetate 6 33.

v .9. A sealing, composition including a mixture of the vfollowing ingredients in the approximate proportions stated:

Parts by weight Percent l 3. 5 10 34. 5 12 41. 3 'loluo 3 10. 3 Butyl acetate 3 l0. 4

10. A sealing composition including a mixture of the following ingredients in the approximate.

proportions stated:

Parts by weight, Percent Ethylcellulose 2 5.7 Butyistearate l 27.7 Filler 12 33.3 Ethyl '2 6.6 Toluol 10 2'7. 7

11. A sealing composition including a mixt ur oi the followingingredients in the approximate proportions stated:

I Percent by weight Cellulose nitrate.. ....q... Acetone 8.5 Ethyl acetate 10,

Butyl acetate 4.5

a V 5 of the following ingredients in the approximate Percent by weight proportions stated: Castor oil 30 Per cent Filler (Asbestine) 44 Cellulose ester I 12. Ase'aling composition including, a cellummited solubility is -"f "7"" 5 lose derivative selected from.the, group consist- Fmer in: oi cellulose esters and cellulose ethers in Li physical solution in a liquid solvent, butyl stearate physically dissolved in the-derivative solutlon in excess of the retentivity of the deriva- ;tive, for the butyl stearate, whereby when the liquid so'lventevaporates, the excess of the butyl ,stearate will seaprate from-the derivative and .form a lubricating film oi butyl stearate upon the mass 01! the composition,,while the balance lose derivative selected from the group consisting of cellulose esters and cellulose ethers in physical solution in a liquid solvent, a plasticizer physically soluble in the derivative in limitedproportionsdissolved'in the derivative solution in excess of its solubility inthe derivative, said plasticizer being present in amounts at least five times the amount of the derivative whereby when the liquid solvent evaporates, the excess or, the plasticizerwill separate from the derivative and form a film of plasticizer upon the mass of the composition, while the balance of the plasticizer will remain intimately associated with the derivative and maintain the mass oi'the composition ina plastic condition.

14. A sealing composition including, a cellulose derivative selected from the group consisting of cellulose esters and cellulose ethers in physical solution in a liquid solvent, a plasticizerphysicallysoluble in the derivative in limited propor- I tions dissolved in the derivative solution in ex-' cess or its solubility in the derivative and being in excess of the ratio 01 5 to 1 with respect to said derivative, whereby the excess of the plas- 4 ticizer will separate from the derivative and form a film of plasticizer upon the massfor the composition and the balance or the plastioizer-will remain intimately associatedwith the derivative and maintainthe mass otthe composition in a plastic condition upon evaporation or the liquid m solvent.

.- LAURENCE L. REC'I'OR.

CHARLES L. CRON. 

